Triethylamine → 2-(methylthio)-N-(2-methylpent-3-yn-2-yl)acetamide

HRID 563887노트

반응식

HRID 563887 반응식
C(N([CH2:6][CH3:7])CC)C.Cl.[NH2:9][C:10]([CH3:15])([CH3:14])[C:11]#[C:12][CH3:13].CC[C:18](O)=[S:19].C1C=CC2N([OH:30])N=NC=2C=1>CN(C=O)C.O.C(Cl)CCl>[CH3:18][S:19][CH2:6][C:7]([NH:9][C:10]([CH3:15])([C:11]#[C:12][CH3:13])[CH3:14])=[O:30]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 219231292-Methylpent-3-yn-2-amine hydrochlorideHCID 178460587HCID 178460587, 화합물

생성물 1

HCID 860149882-(methylthio)-N-(2-methylpent-3-yn-2-yl)acetamide

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

Triethylamine (1.84 ml) was added to a stirred solution of 4-amino-4-methyl-pent-2-yne hydrochloride (1.278 g) in DMF (5 ml) giving a white suspension. Methylthioacetic acid (1.0 g) in DMF (5 ml) was then added to the amine followed by the HOBT (1.27 g) and finally EDC (1.806 g). The white suspension was stirred at ambient temperature for 6 hours, and stored for 18 hours. Water was added and the aqueous phase was extracted with diethyl ether. The organic phases were combined, washed with water and dried over magnesium sulphate then filtered and evaporated to give 2-(methylthio)-N-(2-methylpent-3-yn-2-yl) acetamide as a yellow orange solid (1.9 g).

후처리

  1. customgiving a white suspension
  2. waitstored for 18 hours
  3. extractionthe aqueous phase was extracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationthen filtered
  7. customevaporated

출처 및 근거

ORD 기록
ord-ebacb50a592d4e359ac795237b12617b
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067592B2

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